Layered double hydroxides having different cationic (Mg2+, Co2+, Al3+) composition were successfully synthesized by the low supersaturation method. The samples were thermally decomposed and reconstructed using water and nitrate media at different temperatures. X-ray powder diffraction analysis, X-ray fluorescence analysis, thermogravimetry and BET/BJH methods were used to investigate the differences between the directly obtained layered materials and those after the reconstruction process.